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Cyclohexanol → Cyclohexyl 5-(2,4-dichlorophenoxy)-2-nitrobenzoate

HRID 1414148
ノート
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反応式

HRID 1414148 の反応式
[CH:1]1([OH:7])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.C(N(CC)CC)C.[Cl:15][C:16]1[CH:34]=[C:33]([Cl:35])[CH:32]=[CH:31][C:17]=1[O:18][C:19]1[CH:20]=[CH:21][C:22]([N+:28]([O-:30])=[O:29])=[C:23]([CH:27]=1)[C:24](Cl)=[O:25].Cl.C(N(CC)CC)C>C1(C)C=CC=CC=1.C(OCC)C>[Cl:15][C:16]1[CH:34]=[C:33]([Cl:35])[CH:32]=[CH:31][C:17]=1[O:18][C:19]1[CH:20]=[CH:21][C:22]([N+:28]([O-:30])=[O:29])=[C:23]([CH:27]=1)[C:24]([O:7][CH:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1)=[O:25]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 7966CyclohexanolHCID 8471TriethylamineHCID 11130Triethylamine hydrochlorideHCID 130202985-(2,4-Dichlorophenoxy)-2-nitrobenzoyl chloride

生成物 1

HCID 21486094Cyclohexyl 5-(2,4-dichlorophenoxy)-2-nitrobenzoate

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒
HCID 3283Diethyl Ether溶媒

実験手順

To a stirred solution of cyclohexanol (1.05g., 0.0105 mole) and triethylamine (1.10g., 0.011 mole) in toluene (30 ml.) was added 5-(2',4'-dichlorophenoxy)-2-nitrobenzoyl chloride (3.47g., 0.01 mole). A precipitate of triethylamine hydrochloride occurred immediately. The reaction solution was heated to reflux for one hour, cooled and diluted with diethyl ether (150 ml.). After filtering the triethylamine hydrochloride, the solvent was evaporated to give 4.1g. of a brown oil. A small amount of additional precipitate was filtered off. The ether was again stripped to yield 3.5g. of brown oil.

後処理

  1. temperatureThe reaction solution was heated
  2. temperatureto reflux for one hour
  3. temperaturecooled
  4. filtrationAfter filtering the triethylamine hydrochloride
  5. customthe solvent was evaporated
  6. customto give 4.1g
  7. filtrationA small amount of additional precipitate was filtered off
  8. customto yield 3.5g

出典と根拠

ORDレコード
ord-c9e2f7d53ff048e39212d9718131f103
出典データセット
uspto-grants-1977_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04001005

反応ノート

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